Department of Chemistry and Chemical Engineering, Inha University, Incheon, 402-701, South Korea.
Anal Bioanal Chem. 2021 Jul;413(16):4329-4339. doi: 10.1007/s00216-021-03389-2. Epub 2021 May 26.
A reliable and efficient method for the simultaneous extraction and determination of antibiotics of ciprofloxacin and levofloxacin from milk was developed with solid phase extraction based on tailored adsorbent materials of deep eutectic solvents modified phenolic resin (DES-R-SPE). Six types of polyhydric alcohol-based hydrophilic DESs were prepared to modify the phenolic resin with the compositions of 3-aminophenol as a functional monomer, glyoxylic acid as a crosslinker, and polyethylene glycol 6000 as a porogen. And the prepared DES-Rs showed better extraction capacities for the target analytes than the unmodified phenolic resin because of more hydrogen bonding and electrostatic interactions supplied by DESs. The choline chloride-glycerol-based resin (DES-R) with the highest adsorption amounts was selected and the adsorption behavior of it was studied with static adsorption and the dynamic adsorption performance; the adsorption process followed Freundlich isotherm (R ≥ 0.9337) and pseudo-second-order (R ≥ 0.9951). The present DES-R-SPE method showed good linear range from 0.5 to100 μg mL (R ≥ 0.9998), good recoveries of spiked milk samples (LEV, 96.7%; CIP, 101.5%), and satisfied repeatability for intra-day and inter-day (LEV, RSD≤5.4%; CIP, RSD≤4.6%).
建立了一种基于深共晶溶剂改性酚醛树脂(DES-R-SPE)的固相萃取,用于同时从牛奶中提取和测定环丙沙星和左氧氟沙星抗生素的可靠、高效方法。制备了六种多元醇基亲水性深共晶溶剂,以 3-氨基酚为功能单体、乙醛酸为交联剂、聚乙二醇 6000 为致孔剂改性酚醛树脂。由于 DES 提供了更多的氢键和静电相互作用,所制备的 DES-R 对目标分析物具有更好的萃取能力。选择吸附量最高的氯化胆碱-甘油基树脂(DES-R),并通过静态吸附和动态吸附性能研究其吸附行为;吸附过程遵循弗伦德利希等温线(R≥0.9337)和拟二级动力学(R≥0.9951)。本研究中的 DES-R-SPE 方法在 0.5 至 100 μg mL 范围内表现出良好的线性范围(R≥0.9998),对牛奶样品的加标回收率良好(LEV,96.7%;CIP,101.5%),日内和日间重复性良好(LEV,RSD≤5.4%;CIP,RSD≤4.6%)。